CN106517115A - Method for preparing graphite phase carbon nitride nanosheet through airtight oxidation - Google Patents
Method for preparing graphite phase carbon nitride nanosheet through airtight oxidation Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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Abstract
The invention discloses a method for preparing a graphite phase carbon nitride nanosheet through airtight oxidation. The method comprises the following steps: with a layered graphite phase carbonitride material as a raw material, putting the layered graphite phase carbonitride material, potassium permanganate and concentrated sulfuric acid in an enclosed reaction vessel with a polytetrafluoroethylene lining for a pressurized oxidation reaction so as to obtain oxidized graphite phase carbon nitride; removing unreacted potassium permanganate with hydrogen peroxide; carrying out washing with hydrochloric acid and distilled water; and then carrying out drying so as to obtain the graphite phase carbon nitride nanosheet. Compared with conventional methods, the method provided by the invention has the advantages of less operation steps, low temperature requirement and short reaction time. The prepared graphite phase carbon nitride nanosheet has high purity and few structural defects and has extensive application prospects in fields like heterogeneous catalysis, photocatalysis and biological imaging.
Description
Technical field
The present invention relates to a kind of preparation method of graphite phase carbon nitride nanometer sheet, and in particular to one kind utilizes politef
The quick method for preparing graphite phase carbon nitride nanometer sheet of closed pressure oxidation reaction in liner reactor.
Technical background
There is five kinds of allotropes, i.e. Alpha's phase, beta phase, Emission in Cubic, quasi- Emission in Cubic and graphite in carbon nitride material
Phase.Wherein graphite phase carbon nitride, i.e. g-C3N4It is most stable of one kind.g-C3N4Because its good chemical stability, unique half
Conductor band structure, nontoxic and raw material be easy to get, without the excellent specific properties such as metal photocatalysis contaminant degradation, photolysis water hydrogen,
The fields such as photocatalysis organic synthesiss get more and more people's extensive concerning.But g-C3N4Some be there are as a kind of photocatalyst to lack
Point, such as specific surface area are little, the exciton binding energy of photo-generated carrier high, photo-generate electron-hole is combined serious, visible light utilization efficiency
The low further raising for limiting graphite phase carbon nitride material property.
The research and application of graphite phase carbon nitride nanometer sheet depends on which extensive and inexpensive preparation, current graphite-phase
The preparation method of azotized carbon nano piece mainly has four kinds：(1) chemical oxidization method：Graphite phase carbon nitride material and other materials are acted on
When by the dioxygen oxidation in air so that reaction force attenuation between layers and interlayer structure will not be destroyed.So as to C-N is former
Sublayer can gradually from block g-C3N4On come off so as to more and more thinner is so as to obtaining g-C3N4Nanometer sheet [Niu, P., Zhang,
L.L.,Liu,G.and Cheng,H.M.(2012)Graphene-like carbon nitride nanosheets for
improved photocatalytic activities.Advanced Functional Materials,22,4763-
4770.].Chemical oxidization method is low for equipment requirements, the g-C that yield is high but resulting3N4Nanometer sheet degree of crystallinity is not high, size is little and
And nanometer sheet thickness is wayward, therefore can only be used for synthesizing g-C of low quality3N4Nanometer sheet.(2) prepared by liquid phase stripping method
g-C3N4Nanometer sheet [Zhao, H.X., Yu, H.T., Quan, X., Chen, S.and Zhang, Y.B. (2014) Fabrication
of atomic single layer graphitic-C3N4and its high performance of
photocatalytic disinfection under visible light irradiation.Applied Catalysis
B:Environmental,152,46-50.].Although obtained nanometer sheet thickness is little, and it is complete to maintain body phase material
Crystal structure and identical chemical composition, but the shortcomings of there is cumbersome, long preparation period, high cost in liquid phase separation method.
Therefore this method is not suitable for industrially producing g-C3N4 nanometer sheet in enormous quantities, is only used for laboratory synthesis.(3) gas is dredged
Song Fa:Body phase material is made to become soft while producing many using a large amount of gases that reactant is constantly produced during the course of the reaction
A kind of method [Dong, F., Wu, L.W., Sun, Y.J., Fu, M., Wu, Z.B.and Lee, the S.C. (2011) of pore structure
Efficient synthesis of polymeric g-C3N4layered materials as novel efficient
visible light driven photocatalysts.Journal of Materials Chemistry,21,15171-
15174.].(4) a kind of magnanimity prepares the method [Chinese Patent Application No. of graphite phase carbon nitride nanometer sheet：
201410115068.4]：The method with lamellar graphite phase carbon nitride material as raw material, with compared with eutectic point melting be combined
Alkali metal hydroxide is peeled off to graphite phase carbon nitride, prepares graphite phase carbon nitride nanometer sheet at low temperature.The present invention is carried
For preparation method in, raw material is cheap and easy to get, and process safety is simple, and preparation condition is gentle, is adapted to low cost magnanimity and prepares graphite
Phase carbon nitride nanometer sheet.The two-dimentional graphite phase carbon nitride nanometer sheet purity height of preparation, size uniform, in heterogeneous catalysiss, photocatalysis
It is with a wide range of applications with the field such as bio-imaging.
The content of the invention
The invention provides the quick preparation of closed pressure oxidation reaction in a kind of utilization polytetrafluoroethyllining lining reactor
The method of graphite phase carbon nitride nanometer sheet.
Present invention solves the technical problem that being to provide one kind rapidly and efficiently to prepare high-quality graphite phase carbon nitride nanometer sheet
Method, the method step is few, takes short, and product structure defect is few, and yield is high.Solve
The shortcomings of rapid loaded down with trivial details, time consumption and energy consumption, low yield.
The present invention it is critical that employ the mode of closed oxidation, the gas produced on the one hand can preventing from reacting
Body is escaped, so that reaction is carried out in the state of being in a pressurization, effectively raises the product of graphite phase carbon nitride nanometer sheet
Rate, shortens the response time；On the other hand the loss of material in course of reaction also can effectively be prevented.Additionally, closed reactor
Using can also make whole preparation process safer and simpler, the danger that the reagents such as concentrated sulphuric acid, potassium permanganate bring is overcome.
According to the present invention, the preparation process of graphite phase carbon nitride nanometer sheet is as follows：
(1) using a kind of jacket reactor as reaction vessel, kettle (containing kettle cover) is stainless steel, and liner is poly- four
Fluorothene material, the reactor provide the reaction compartment of security closed for reaction；By the reactor and graphite phase carbon nitride, Gao Meng
Cold preservation at least three hours in sour potassium, concentrated sulphuric acid, graduated cylinder placement refrigerator (0-5 DEG C)；
(2) raw material in step (1) is taken out from refrigerator, 0.6g graphite is sequentially added in polytetrafluoroethyllining lining
Phase carbon nitride, 3g potassium permanganate, 30ml concentrated sulphuric acids.Stainless steel cauldron is tightened, cold preservation 1.5h in refrigerator (0-5 DEG C) is placed.Take
Tighten reactor after going out again and place heating 1.5h in baking oven (80 DEG C).Reactor is taken out afterwards is cooled to room temperature；
(3) pour the product in polytetrafluoroethyllining lining in 400ml distilled water (stirring of side bevelling), be subsequently adding 30%
Hydrogen peroxide (stirring of side bevelling), until solution becomes pure white and stops adding.Finally washed with 5% hydrochloric acid and deionized water centrifugation
Wash to neutrality, place drying or lyophilization in baking oven (60 DEG C).
In above-mentioned technical proposal described in step (1) raw material is placed refrigerator (0-5 DEG C) in cold preservation at least three it is little
When, it is to ensure that raw materials used in cold state, can so reduces the danger that the reagents such as potassium permanganate, concentrated sulphuric acid bring.
When in above-mentioned technical proposal add various raw materials in polytetrafluoroethyllining lining, operation must
Hurry up, be to ensure that raw materials used in cold state, can so reduce the danger that the reagents such as potassium permanganate, concentrated sulphuric acid bring.
Stainless steel cauldron must be tightened in step (2) in above-mentioned technical proposal, be conducive to graphite phase carbon nitride abundant
Oxidation.
Reactor is placed into cold preservation 1.5h in refrigerator (0-5 DEG C) in step (2) in above-mentioned technical proposal, is then twisted again
Tight reactor places heating 1.5h in baking oven (80 DEG C).It is that graphite phase carbon nitride to be allowed both had experienced low-temperature oxidation and experienced high temperature oxygen
Change so as to more fully oxidized.
Hydrogen-peroxide reduction manganese ion is added in above-mentioned technical proposal in step (3) intermediate product, unreacted height is removed
Potassium manganate, it is to avoid excessive exothermic in washing process.
In above process, concentrated sulphuric acid ensure that reaction in anhydrous state, but the presence of concentrated sulphuric acid can increase product
The separating, washing difficulty of thing, it is therefore desirable to which substantial amounts of hydrochloric acid and deionized water are washed.With salt acid elution to PH>5, use
Deionized water wash is to neutrality.
Hydrochloric acid 600ml used during centrifuge washing in step (3) in above-mentioned technical proposal, centrifuge washing rotating speed are 10000r/
Min, each 3min, are centrifuged 4-5 time altogether.
Centrifuge washing when institute deionized water 1000ml in step (3) in above-mentioned technical proposal, centrifuge washing rotating speed is
10000r/min, each 3min, are centrifuged 6-7 time altogether.
It should be noted that the use of the purpose of potassium permanganate and concentrated sulphuric acid being to destroy graphite phase carbon nitride as oxidant
C-N keys, make graphite phase carbon nitride longitudinally slit, obtain the graphite phase carbon nitride of planar structure.Optimum potassium permanganate and stone
The mass ratio of black phase carbon nitride is 5：1.
It should be noted that being to provide the closed environment needed for reaction using the purpose of polytetrafluoroethyllining lining reactor, protect
Card reaction is carried out under pressure, and is prevented material such as potassium permanganate as gas seethes with excitement and lost, and improves reaction efficiency
And yield, shorten the response time.
Preferably, in above-mentioned steps (1) and (2), refrigerator temperature is set to 0-5 DEG C.
Preferably, when above-mentioned steps (2) high temperature is aoxidized, oven temperature is set to 80 DEG C.
Preferably, when wet graphite phase carbon nitride nanometer sheet is dried in above-mentioned steps (3), oven temperature is set to 60 DEG C.
Preferably, in above-mentioned steps (3), the mass fraction of hydrogen peroxide is 30%, and hydrochloric acid mass fraction is 5%.
The present invention except pattern is good with can be prepared on a large scale out, the high graphite phase carbon nitride nanometer sheet of quality.Also have
Have the advantage that：(1) graphite phase carbon nitride nanometer sheet can be quickly prepared, method is simple, and low cost, yield are high；(2) prepared
Addition without any surfactant and organic reagent in journey, and using closed reaction kit, environmental protection；(3) prepared
In journey, degree of oxidation is easily controlled and takes short.
Description of the drawings
Fig. 1 is the Tyndall effect that graphite phase carbon nitride nanometer sheet laser irradiation prepared by the present invention is produced；
Fig. 2 is the transmission electron microscope (TEM) of graphite phase carbon nitride nanometer sheet prepared by the present invention；
Fig. 3 is the fluorogram (FL) of graphite phase carbon nitride nanometer sheet prepared by the present invention.
Specific embodiment
The present invention is described in further detail below by specific embodiments and the drawings.It is concrete listed by the present invention
Embodiment is only limitted to the explanation present invention, rather than limitation of the invention.
Embodiment 1
0.6g graphite phase carbon nitrides, 3g potassium permanganate, 30ml concentrated sulphuric acids are sequentially added in polytetrafluoroethyllining lining.Tighten
Stainless steel cauldron, it is closed, place cold preservation 1.5h in refrigerator (0-5 DEG C).Tighten reactor after taking out again and place baking oven (80
DEG C) middle heating 1.5h.Reactor is taken out afterwards is cooled to room temperature.Diluted with 400ml deionized waters, side stirring does not add 30% mistake
Hydrogen oxide, until solution becomes pure white and stops adding.Finally with 5% hydrochloric acid of 600ml and 1000ml deionized water wash into
Property, place drying in baking oven (60 DEG C).
Fig. 1 is the laser figure of graphite phase carbon nitride nanometer sheet prepared by the present invention, it will be seen from figure 1 that obtained by experiment
Product laser irradiation can produce Tyndall effect, illustrate the size of product between 1-100nm, be that graphite phase carbon nitride is received
Rice piece.
Embodiment 2
0.6g graphite phase carbon nitrides, 3g potassium permanganate, 30ml concentrated sulphuric acids are sequentially added in polytetrafluoroethyllining lining.Tighten
Stainless steel cauldron, it is closed, place cold preservation 1.5h in refrigerator (0-5 DEG C).Tighten reactor after taking out again and place baking oven (80
DEG C) middle heating 1.5h.Reactor is taken out afterwards is cooled to room temperature.Diluted with 400ml deionized waters, side stirring does not add 30% mistake
Hydrogen oxide, until solution becomes pure white and stops adding.Deionized water filtering and washing is dried in placing baking oven (60 DEG C) to neutrality
It is dry.Obtain 100mg graphite phase carbon nitride nanometer sheet.
Fig. 2 is the transmission electron microscope (TEM) of graphite phase carbon nitride nanometer sheet prepared by the present invention.
Embodiment 3
0.6g graphite phase carbon nitrides, 3g potassium permanganate, 30ml concentrated sulphuric acids are sequentially added in polytetrafluoroethyllining lining.Tighten
Stainless steel cauldron, it is closed, place cold preservation 1.5h in refrigerator (0-5 DEG C).Tighten reactor after taking out again and place baking oven (80
DEG C) middle heating 1.5h.Reactor is taken out afterwards is cooled to room temperature.Diluted with 400ml deionized waters, side stirring does not add 30% mistake
Hydrogen oxide, until solution becomes pure white and stops adding.Finally with 600ml5% hydrochloric acid and 1000ml deionized water wash into
Property, carry out lyophilization.
Fig. 3 is the fluorogram (FL) of graphite phase carbon nitride nanometer sheet prepared by the present invention, from figure 3, it can be seen that graphite
The fluorescence intensity of the fluorescence intensity ratio graphite phase carbon nitride of phase carbon nitride is remarkably reinforced.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (8)
1. a kind of method that closed oxidizing process prepares graphite phase carbon nitride nanometer sheet, it is characterised in that comprise the following steps：
(1) using a kind of jacket reactor as reaction vessel, kettle (containing kettle cover) is stainless steel, and liner is polytetrafluoroethyl-ne
Alkene material, the reactor provide the reaction compartment of security closed for reaction, by the reactor and graphite phase carbon nitride, permanganic acid
Cold preservation at least three hours in potassium, concentrated sulphuric acid, graduated cylinder placement refrigerator (0-5 DEG C)；
(2) above-mentioned raw material is taken out from refrigerator, 0.6g graphite phase carbon nitrides, 3g is sequentially added in polytetrafluoroethyllining lining
Potassium permanganate, 30ml concentrated sulphuric acids.Stainless steel cauldron is tightened, cold preservation 1.5h in refrigerator (0-5 DEG C) is placed.Tightened after taking out again
Reactor places heating 1.5h in baking oven (80 DEG C).Reactor is taken out afterwards is cooled to room temperature；
(3) pour the product in polytetrafluoroethyllining lining in 400ml deionized waters (stirring of side bevelling), be subsequently adding 30% mistake
Hydrogen oxide (stirring of side bevelling), until solution becomes pure white and stops adding.Finally with 5% hydrochloric acid and deionized water wash into
Property, place drying or lyophilization in baking oven (60 DEG C).
2. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
Used in step (1), ptfe autoclave provides the reaction compartment of security closed for reaction.
3. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
Raw material is placed into cold preservation at least three hours in refrigerator (0-5 DEG C) before the reaction in step (2), it is ensured that raw materials used in cold
State.
4. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
In step (2), the mass ratio of potassium permanganate and graphite phase carbon nitride is 5：1.
5. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
When step (2) high temperature is aoxidized, oven temperature is set to 80 DEG C.
6. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
In step (3), the mass fraction of hydrogen peroxide used is 30%, and the mass fraction of hydrochloric acid used by washed product is 5%.
7. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
When wet graphite phase carbon nitride nanometer sheet is dried in step (3), oven temperature is set to 60 DEG C.
8. a kind of method that closed oxidation prepares graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that
With salt acid elution to PH in step (3)>5, it is washed with deionized to neutrality.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190849A (en) * | 2017-12-28 | 2018-06-22 | 四川大学 | A kind of graphite phase carbon nitride nanoparticle and preparation method thereof |
| CN108816286A (en) * | 2018-04-11 | 2018-11-16 | 湖北大学 | A kind of Cu-Ag/g-C3N4The preparation method of/ZIF tri compound analogue enztme |
| CN110143578A (en) * | 2019-04-19 | 2019-08-20 | 南通途纳新材料有限公司 | The preparation method of graphite phase carbon nitride |
| CN110176362A (en) * | 2019-06-19 | 2019-08-27 | 内蒙古民族大学 | A kind of self-supported membrane stacked electrodes and preparation method thereof and a kind of fake capacitance supercapacitor |
| CN110697666A (en) * | 2019-09-17 | 2020-01-17 | 中国科学技术大学 | Graphite oxide phase carbon nitride and preparation method and application thereof |
| CN115636984A (en) * | 2022-10-31 | 2023-01-24 | 嘉兴学院 | Application of oxidized carbon nitride nanosheet in tough heat-resistant epoxy resin composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108190849A (en) * | 2017-12-28 | 2018-06-22 | 四川大学 | A kind of graphite phase carbon nitride nanoparticle and preparation method thereof |
| CN108190849B (en) * | 2017-12-28 | 2021-09-14 | 四川大学 | Graphite phase carbon nitride nano particle and preparation method thereof |
| CN108816286A (en) * | 2018-04-11 | 2018-11-16 | 湖北大学 | A kind of Cu-Ag/g-C3N4The preparation method of/ZIF tri compound analogue enztme |
| CN110143578A (en) * | 2019-04-19 | 2019-08-20 | 南通途纳新材料有限公司 | The preparation method of graphite phase carbon nitride |
| CN110143578B (en) * | 2019-04-19 | 2022-09-23 | 南通途纳新材料有限公司 | Preparation method of graphite phase carbon nitride |
| CN110176362A (en) * | 2019-06-19 | 2019-08-27 | 内蒙古民族大学 | A kind of self-supported membrane stacked electrodes and preparation method thereof and a kind of fake capacitance supercapacitor |
| CN110697666A (en) * | 2019-09-17 | 2020-01-17 | 中国科学技术大学 | Graphite oxide phase carbon nitride and preparation method and application thereof |
| CN110697666B (en) * | 2019-09-17 | 2021-08-13 | 中国科学技术大学 | Graphite oxide phase carbon nitride and preparation method and application thereof |
| CN115636984A (en) * | 2022-10-31 | 2023-01-24 | 嘉兴学院 | Application of oxidized carbon nitride nanosheet in tough heat-resistant epoxy resin composite material |
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| CN106517115B (en) | 2019-06-25 |
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